Structure and corrosion behavior of FeCoCrNiMo high-entropy alloy coatings prepared by mechanical alloying and plasma spraying

FeCoCrNiMox composite powders were prepared using the mechanical alloying technique and made into high-entropy alloy(HEA)coatings with the face-centered cubic phase using plasma spraying to address the element segregation problem in HEAs and pre-pare uniform HEA coatings.Scanning electron microscopy,transmission electron microscopy,and X-ray diffractometry were employed to characterize these coatings’microstructure and phase composition.The hardness,elastic modulus,and fracture toughness of coatings were tested,and the corrosion resistance was analyzed in simulated seawater.Results show that the hardness of the coating is HV0.1606.15,the modulus of elasticity is 128.42 GPa,and the fracture toughness is 43.98 MPa·m^(1/2).The corrosion potential of the coating in 3.5wt%NaCl solution is-0.49 V,and the corrosion current density is 1.2×10^(−6)A/cm^(2).The electrochemical system comprises three parts:the electrolyte,the adsorption and metallic oxide films produced during immersion,and the FeCoNiCrMo HEA coating.Over in-creasingly long periods,the corrosion reaction rate increases first and then decreases,the corrosion product film comprising metal oxides reaches a dynamic balance between formation and dissolution,and the internal reaction of the coating declines.

Structure and Magnetic Properties of Nd(Fe,Mo)_(12)N_x Prepared by Mechanically Alloying

Nd(Fe,Mo) 12 N x compound with ThMn 12 structure was successfully prepared by mechanically alloying and annealed at the temperature ranging from 750 to 950 ℃ and then nitrided. The structure, formation condition and magnetic properties of compounds were studied using X ray diffraction, TEM and magnetic measurements. Compared to other nitrides with a ThMn 12 structure, the good condition of phase formation and high magnetic properties of Nd(Fe, Mo) 12 N x compounds reveal that it may be a potential candidate for permanent magnets.

Mechanically Driven Alloying and Structural Evolution of Nanocrystalline Fe_(60)Cu_(40) Powder

Highly supersaturated nanocrystalline fcc Fe60Cu40 alloy has been prepared by mechanical alloying of elemental powders. The phase transformation is monitored by X-ray diffraction (XRD),Mossbauer spectroscopy and extended X-ray absorption fine structure (EXAFS). The powder obtained after milling is of single fcc structure with grain size of nanometer order. The Mossbauer spectra of the milled powder can be fitted by two subspectra whose hyperfine magnetic fields are 16 MA/m and 20 MA/m while that of pure Fe disappeared. EXAFS results show that the radial structure function (RSF) of Fe K-edge changed drastically and finally became similar to that of reference Cu K-edge, while that of Cu K-edge nearly keeps unchanged in the process of milling. These imply that bcc Fe really transforms to fcc structure and alloying between Fe and Cu occurs truly on an atomic scale. EXAFS results indicate that iron atoms tend to segregate at the boundaries and Cu atoms are rich in the fcc lattice. Annealing experiments show that the Fe atoms at the interfaces are easy to cluster to α-Fe at a lower temperature, whereas the iron atoms in the lattice will form γ-Fe first at temperature above 350℃, and then transform to bcc Fe

STRUCTURAL TRANSFORMATION INDUCED BY MECHANICALLY DRIVEN ALLOYING AND SUBSEQUENT MAGNETIC PROPERLIESOF THE Fe-Cu SYSTEM

The structural transformation in Fe-Cu powder induced by mechanically driven alloying has been monitored by the lattice constant measurements and Mossbauer spectroscopy. For the samples with Cu higher than 75at.% Mossbauer the spectra show a broad paramagnetic doublet; for samples with 50 and 60at.%Cu a new broad ferromagnetic sextet; for those with less than 30at.%Cu similar to those of α-Fe. The main peaks of the hyperfine field distribution significantly broaden and shift to a lower position with increasing Cu content due to the complex environments of iron atoms in the solid solutions and the reduction in the nearest neighbor Fe of a cental Fe atom, respectively. The saturation magnetization of Fe-Cu alloys monotonously decreases with Cu content. The complex composition dependence of coercive field for the milled samples is discussed with respect to the solid dissolution, grain size, interfacial state etc.. The increase of lattice constants with the solute content in the two terminal solid solutions has been explained by the volume-size factor theory or magnetovolume effect.

Influences of Milling Time and NbC on Microstructure of AlCoCrFeNi_(2.1)High Entropy Alloy by Mechanical Alloying

AlCoCrFeNi_(2.1)eutectic high entropy alloy(EHEA)and AlCoCrFeNi_(2.1)-x NbC(x=2.5wt%,5.0wt%,7.5wt%,and 10wt%)high entropy alloy(HEAs)were prepared by mechanical alloying(MA).The effects of milling time and NbC content on the alloying behavior and grain size of the AlCoCrFeNi_(2.1)EHEA were investigated.The experimental results show that the AlCoCrFeNi_(2.1)EHEA primarily consists of order BCC(B2)and face-centered-cubic(FCC)phases,while the AlCoCrFeNi_(2.1)-x NbC(x=2.5wt%,5.0wt%,7.5wt%,and 10wt%)HEAs are composed of B2,FCC,and NbC phases.With the increase of milling time,the powder goes through three stages,irregularity,cold welding fracture and spheroidization.The particle size of AlCoCrFeNi_(2.1)EHEA powder shows a trend of first increasing and then decreasing.Therein,the particle size presents a normal distribution during 0-50 h alloying.With the addition of NbC,the AlCoCrFeNi_(2.1)-x NbC HEAs powders are significantly refined.And the degree of grain refinement gradually increases with the increase of NbC content.

Rapid synthesis of Ti(C,N) powders by mechanical alloying and subsequent arc discharging

Ti（C,N） powders were synthesized by mechanical alloying （MA） from a mixture of pure titanium and graphite under a nitrogen atmosphere in a planetary mill.Effects of arc discharging on phase transformation and microstructure of MA powders milled for 1-7 h were explored.The results show that Ti（C,N） powders were prepared after mechanical milling for 1 h and subsequent arc discharge treatment,whereas the synthesis reaction did not occur in 7 h by mechanical milling alone.The ions produced during arc discharging interacted with powder particles and accelerated the diffusion of atoms and the nucleation on the surface of the as-milled powder,which results in fast synthesis of Ti（C,N） powders.The formation mechanisms of the two synthesis processes are self-propagating reactive synthesis.

Effect of mechanical alloying and sintering process on microstructure and mechanical properties of Al-Ni-Y-Co-La alloy

Al86Ni7Y4.5Co1La1.5 （mole fraction, %） alloy powder was produced by argon gas atomization process. After high-energy ball milling, the powder was consolidated by vacuum hot press sintering and spark plasma sintering （SPS） under different process conditions. The microstructure and morphology of the powder and consolidated bulk sample were examined by X-ray diffraction （XRD）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. It is shown that amorphous phase appears when ball milling time is more than 100 h, and the bulk sample consolidated by SPS can maintain amorphous/ nanocrystalline microstructure but has lower relative density. A compressive strength of 650 MPa of Al86Ni7Y4.5Co1La1.5 nanostructured samples is achieved by vacuum hot extrusion （VHE）.

Mechanical alloying and phase transformation in Fe-Si alloy

The Fe-Si mechanical alloying and its transformation are investigated to evaluate whether mechanical alloying is a useful process for producing Fe-Si alloy. The mechanical alloying process of Fe-Si powders is studied by SEM（ scanning electron microscopy）, EDS（energy dispersive spectrometer）and XRD（X-ray diffraction）. The results show that the ball milling process first makes tough Fe powder a lump structure and brittle Si powder a small particle, and then as the mill power increases, the tough powder of iron with a lamellar structure forms and the Si particles lies on or between the Fe lamellas. Finally, the Fe and Si powders are mechanically alloyed through atom diffusion. So the Fe and Si powders can be alloyed by 15 h ball milling at a speed of 400 r/min and with a ball-to-powder ratio of 40 ： 1. After heating at 1 243 K for 1 h, the milled powders transform to α-FeSi2, and after heating at 1 243 K for 1 h, then cooling to 1 073 K for 1 h, the milled powders transform to β-FeSi2. Therefore, the monophase α-FeSi2 or β-FeSi2 can be obtained by heat treatment of mechanically alloyed Fe-Si powders.

Pressure sintering of W-15wt.%Cu alloys prepared by mechanical alloying as a subsequent densification treatment method

The sintered W-15wt.%Cu alloys fabricated by mechanical alloying were re-sintered under pressure to increase the density and improve the properties of these alloys. The pressure was applied vertically along the axis of the sintered sample. Properties such as density, hardness, and bending strength were measured. The microstructures of the sintered bodies were observed. The results showed that the subsequent pressure sintering could increase the density of the sintered W-15wt.%Cu alloys. Their hardness, bending strength, and some other physical properties were also improved by this subsequent densification treatment.

Effects of rare earth La on the microstructure and melting property of(Ag-Cu_(28))-30Sn alloys prepared by mechanical alloying

To obtain novel intermediate temperature alloy solders with a melting temperature of 400-600°C,nominal（Ag-Cu28）-30Sn alloys without or with a trace addition（0.5 or 1.0 wt.%） of rare earth（RE） element La were prepared by mechanical alloying.The aim of this research is to investigate the effects of the addition of La on the microstructures,alloying process and melting properties of（Ag-Cu28）-30Sn alloys.The results show that the addition of La produces no new phase.A trace amount of La addition can effectively refine the grain size,but the excessive addition of 1.0 wt.% La inhibits the alloying process.The influence of La on the melting temperatures of solder alloys is negligible.However,the trace addition of 0.5 wt.% La can distinctly reduce the fusion zone and improve the melting property of（Ag-Cu28）-30Sn alloys.

Structural characteristics and magnetic properties of bulk nanocrystalline Fe_(84)Zr_2Nb_4B_(10) alloy prepared by mechanical alloying and spark plasma sintering consolidation

Magnetic properties of Fe84Zr2Nb4B10 sample were investigated. The sample was produced from nanocrystalline powders made by the mechanical alloying (MA) and consolidation using the spark plasma sintering (SPS) technique. Effects of milling time on phase transformation, structural characteristics, and magnetic properties of powders were examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), and physical property measure system (PPMS), respectively. Results show that nanostructured α-Fe supersaturated solid solution is obtained in the final MAed products. The saturation magnetization (Ms) increased with increasing milling time and became constant at 130 h, but the coercivity (Hc) increased firstly and then decreased. The consolidated bulk sample exhibited a high density of 6.893 g·cm-3, there was no phase change during SPS process, and the saturation magnetization and susceptibility of the SPSed bulk sample improved in comparison with the milled powders. The variation of magnetic parameters can be explained by nano-scale effect and Herzer model.

SYNTHESIS OF INTERMETALLICS BY MECHANICAL ALLOYING

Mechanical alloying (MA), a solid-state powder processing method, is a 'far from equilibrium' synthesis technique which allows development of novel crystal structures and microstructures, leading to enhanced physical and mechanical properties. The ability to synthesize a variety of alloy phases including supersaturated solid solutions, nanocrystalline structures, amorphous phases and intermetallic compounds themselves is discussed. No extension of solubility using MA has been observed in the intermetallics studied. Nanostructured grains were observed in all compositions. Long time milling generally resulted in amorphous phase formation in large part because of the increase in grain boundary energy/mole with reduced grain size; good agreement with the Miedema model for amorphization was obtained in the Al-Fe system. Generally an anneal was required to form the intermetallic after MA; however,intermetallics with a large negative enthalpy of formation were detected in the MA condition. A study of the hot isostatic pressing of γ-TiAl powders produced by MA demonstrated that full density can be achieved at least 400℃ below the normal temperature required for conventional powder, that is 725℃ or below. Nanometered sized grains (≤100nm)were observed after HIP'ing up to 850℃.

Microstructure and properties of ultra-fine tungsten heavy alloys prepared by mechanical alloying and electric current activated sintering

The microstructure and properties of the 93W-4Ni-2Co-1Fe(mass fraction,%) tungsten heavy alloys prepared by mechanical alloying and electric current activated sintering from mixed elemental powders were investigated.After 15 h milling,the average W grain size in the powders is decreased to 120 nm.For the powders milled for 15 h,the density,hardness and transverse rupture strength of the alloys sintered only by an intensive pulse electric current are the maximum.When the total sintering time keeps constant,the properties of the sintered alloys can be obviously improved by optimizing the sintering time of pulse-and constant-currents.A bulk ultrafine alloy with an average W grain size of about 340 nm can be obtained by sintering 15 h-milled powders in a total sintering time of 6 min.The corresponding sintered density,hardness and transverse rupture strength reach 16.78 g /cm3,HRA84.3 and 968 MPa,respectively.

Evaluation of the microstructure,thermal and mechanical properties of Cu/SiC nanocomposites fabricated by mechanical alloying

Nano-sized silicon carbide(SiC:0wt%,1wt%,2wt%,4wt%,and 8wt%)reinforced copper(Cu)matrix nanocomposites were manufactured,pressed,and sintered at 775 and 875℃in an argon atmosphere.X-ray diffraction(XRD)and scanning electron microscopy were performed to characterize the microstructural evolution.The density,thermal expansion,mechanical,and electrical properties were studied.XRD analyses showed that with increasing SiC content,the microstrain and dislocation density increased,while the crystal size decreased.The coefficient of thermal expansion(CTE)of the nanocomposites was less than that of the Cu matrix.The improvement in the CTE with increasing sintering temperature may be because of densification of the microstructure.Moreover,the mechanical properties of these nanocomposites showed noticeable enhancements with the addition of SiC and sintering temperatures,where the microhardness and apparent strengthening efficiency of nanocomposites containing 8wt%SiC and sintered at 875℃were 958.7 MPa and 1.07 vol%^(−1),respectively.The electrical conductivity of the sample slightly decreased with additional SiC and increased with sintering temperature.The prepared Cu/SiC nanocomposites possessed good electrical conductivity,high thermal stability,and excellent mechanical properties.

Microstructure Design of High-Entropy Alloys Through a Multistage Mechanical Alloying Strategy for Temperature-Stable Megahertz Electromagnetic Absorption

Developing megahertz(MHz)electromagnetic wave(EMW)absorption materials with broadband absorption,multi-temperature adaptability,and facile preparation method remains a challenge.Herein,nanocrystalline FeCoNiCr_(0.4)Cu_(0.2) high-entropy alloy powders(HEAs)with both large aspect ratios and thin intergranular amorphous layers are constructed by a multistage mechanical alloying strategy,aiming to achieve excellent and temperature-stable permeability and EMW absorption.A single-phase face-centered cubic structure with good ductility and high crystallinity is obtained as wet milling precursors,via precisely controlling dry milling time.Then,HEAs are flattened to improve aspect ratios by synergistically regulating wet milling time.FeCoNiCr_(0.4)Cu_(0.2) HEAs with dry milling 20 h and wet milling 5 h(D20)exhibit higher and more stable permeability because of larger aspect ratios and thinner intergranular amorphous layers.The maximum reflection loss(RL)of D20/SiO_(2) composites is greater than-7 dB with 5 mm thickness,and EMW absorption bandwidth(RL<-7 dB)can maintain between 523 and 600 MHz from-50 to 150℃.Furthermore,relying on the“cocktail effect”of HEAs,D20 sample also exhibits excellent corrosion resistance and high Curie temperature.This work provides a facile and tunable strategy to design MHz electromagnetic absorbers with temperature stability,broadband,and resistance to harsh environments.

Kinetic characteristics of liquid phase sintering of mechanically activated W-15wt%Cu powder

The kinetic characteristics of W grain growth operated by diffusion controlled Oswald ripening （DOR） during liquid phase sintering were studied. A liquid phase sintering of W-15wt%Cu was carried out by pushing compacts into a furnace at the moment when the temperature increased to 1340℃ for different sintering times. The results show that liquid phase sintering produces the compacts with considerably low relative density and inversely, rather high homogeneity. On the basis of the data extracted from the SEM images, the kinetic equation of W grain growth, G^n = G0^n ＋ kt, is determined in which the grain growth exponent n is 3 and the grain growth rate constant k is 0.15 μm^3/s. The cumulative normalized grain size distributions produced by different sintering times show self-similar. The cumulative distribution function is extracted from the curves by non-linear fitting. In addition, the sintering kinetic characteristics of W-15wt%Cu compacts were also investigated.

Microstructure, thermal properties, and corrosion behaviors of FeSiBAlNi alloy fabricated by mechanical alloying and spark plasma sintering

An equiatomic FeSiBAlNi amorphous high-entropy alloy （HEA） was fabricated by mechanical alloying （MA）. A fully amorphous phase was obtained in the FeSiBAlNi HEA after 240 h of MA. The bulk FeSiBAlNi samples were sintered by spark plasma sintering （SPS） at 520 and 1080℃ under a pressure of 80 MPa. The sample sintered at 520℃ exhibited an amorphous composite structure comprising solid-solution phases （body-centered cubic （bcc） and face-centered cubic （fee） phases）. When the as-milled amorphous HEA was consoli- dated at 1080℃, another fcc phase appeared and the amorphous phase disappeared. The sample sintered by SPS at 1080℃ exhibited a slightly higher melting temperature compared with those of the as-milled alloy and the bulk sample sintered at 520℃. The corrosion behav- iors of the as-sintered samples were investigated by potentiodynamic polarization measurements and immersion tests in seawater solution. The results showed that the HEA obtained by SPS at 1080℃ exhibited better corrosion resistance than that obtained by SPS at 520℃.

Alloying behavior and characterization of(CoCrFeNiMn)_(90)M_(10)(M=Al,Hf)high-entropy materials fabricated by mechanical alloying

The alloying behavior and microstructures of the(CoCrFeNiMn)_(90)M_(10)(M=Al,Hf)high-entropy alloy(HEA)powders fabricated by mechanical alloying were studied.The CoCrFeNiMn)_(90)Al_(10) powders have duplex solid-solution structures.In contrast,nanocrystalline HfNi_(3) anchoring in amorphous structures is found in the(CoCrFeNiMn)_(90)Hf_(10) powders.The(CoCrFeNiMn)_(90)Al_(10) powders show better ferromagnetic behaviors,mainly explained by the facilitated motion of the magnetic domain induced by the coherent interface between duplex phases.Combined with our previous work,the rules of forming solid-solution and amorphous phase in as-milled HEA powders are preliminarily proposed.It is found that,compared with the as-cast HEA reported previously,the variation range of mixing enthalpy with atomic size difference of the solid-solution formed in as-milled HEA powders is broader.Moreover,the variation ranges between mixing enthalpy and entropy with atomic size difference of the amorphous phase in HEA powder become wider than those of high-entropy bulk metallic glass.

Influence of B source materials on the synthesis of TiB_2-Al_2O_3 nanocomposite powders by mechanical alloying

An Al2O3-TiB2 nanocomposite was successfully synthesized by ball milling of Al, TiO2 and two B source materials of B2O3 （system （1）） and H3BO3 （system （2））. Phase identification of the milled samples was examined by Xray diffraction. The morphology and microstructure of the milled powders were monitored by scanning electron microscopy and transmission electron microscopy. It was found that the formation of this composite was completed after 15 and 30 h of milling time in systems （1） and （2）, respectively. More milling energy was required for the formation of this composite in system （2） due to the lubricant properties of HaBO3 and also its decomposition to HBO2 and B2O3 during milling. On the basis of X-ray diffraction patterns and thermodynamic calculations, this composite was formed by highly exothermic mechanically induced self-sustaining reactions （MSR） in both systems. The MSR mode took place around 9 h and 25 h of milling in systems （1） and （2）, respectively. At the end of milling （15 h for system （1） and 30 h for system （2）） the grain size of about 35-50 nm was obtained in both systems.

Influence of mechanical alloying time on the properties of Fe_3Al intermetallics prepared by spark plasma sintering

The Fe3Al-based intermetallics were prepared by mechanical alloying and spark plasma sintering （SPS）, and the influence of milling time on the properties of materials was investigated. The phase identification was investigated by X-ray, and the surface morphology and fractography were observed by scanning electron microscope （SEM）. The mechanical properties such as bending strength, strain, and microhardness were tested. The results show that Fe reacts with Al completely to form Fe3Al during short SPS processing time. The relative densities of the sintered samples were nearly 100%. The mechanical properties of the sintered samples can be improved along with the milling time. The representative values are the bend strength of 1327 MPa and the microhardness of 434.